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Study of Chromium Migration in a Nickel-Based Alloy Using Polarized Neutron Reflectometry and Rutherford Backscattering Spectrometry

Journal of Physical Chemistry C

Doucet, Mathieu; Browning, James F.; Doyle, Barney L.; Charlton, Timothy R.; Ambaye, Haile; Seo, Joohyun; Mazza, Alessandro R.; Wenzel, John F.; Burns, George B.; Wixom, Ryan R.; Veith, Gabriel M.

Haynes 230 nickel alloy is one of the main contenders for salt containment in the design of thermal energy storage systems based on molten salts. A key problem for these systems is understanding the corrosion phenomena at the alloy–salt interface, and, in particular, the role played by chromium in these processes. In this study, thin films of Haynes 230, which is also rich in chromium, were measured with polarized neutron reflectometry and Rutherford backscattering spectrometry as a function of annealing temperature. Migration of chromium to the surface was observed for films annealed at 400 and 600 °C. Combining the two techniques determined that more than 60% of chromium comprising the as-prepared Haynes 230 layer moves to the surface when annealed at 600 °C, where it forms an oxide layer.

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Atom Interferometry in a Warm Vapor

Physical Review Letters

Biedermann, Grant B.; McGuinness, Hayden J.; Rakholia, A.V.; Jau, Yuan-Yu J.; Wheeler, David R.; Sterk, J.D.; Burns, George B.

We demonstrate matter-wave interference in a warm vapor of rubidium atoms. Established approaches to light-pulse atom interferometry rely on laser cooling to concentrate a large ensemble of atoms into a velocity class resonant with the atom optical light pulse. In our experiment, we show that clear interference signals may be obtained without laser cooling. This effect relies on the Doppler selectivity of the atom interferometer resonance. This interferometer may be configured to measure accelerations, and we demonstrate that multiple interferometers may be operated simultaneously by addressing multiple velocity classes.

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Modeling injection molding of net-shape active ceramic components

Rao, Rekha R.; Brooks, Carlton F.; Cote, Raymond O.; Castaneda, Jaime N.; Mondy, L.A.; Noble, David R.; Hopkins, Matthew M.; Notz, Patrick N.; Halbleib, Laura L.; Yang, Pin Y.; Burns, George B.; Grillet, Anne M.

To reduce costs and hazardous wastes associated with the production of lead-based active ceramic components, an injection molding process is being investigated to replace the current machining process. Here, lead zirconate titanate (PZT) ceramic particles are suspended in a thermoplastic resin and are injected into a mold and allowed to cool. The part is then bisque fired and sintered to complete the densification process. To help design this new process we use a finite element model to describe the injection molding of the ceramic paste. Flow solutions are obtained using a coupled, finite-element based, Newton-Raphson numerical method based on the GOMA/ARIA suite of Sandia flow solvers. The evolution of the free surface is solved with an advanced level set algorithm. This approach incorporates novel methods for representing surface tension and wetting forces that affect the evolution of the free surface. Thermal, rheological, and wetting properties of the PZT paste are measured for use as input to the model. The viscosity of the PZT is highly dependent both on temperature and shear rate. One challenge in modeling the injection process is coming up with appropriate constitutive equations that capture relevant phenomenology without being too computationally complex. For this reason we model the material as a Carreau fluid and a WLF temperature dependence. Two-dimensional (2D) modeling is performed to explore the effects of the shear in isothermal conditions. Results indicate that very low viscosity regions exist near walls and that these results look similar in terms of meniscus shape and fill times to a simple Newtonian constitutive equation at the shear-thinned viscosity for the paste. These results allow us to pick a representative viscosity to use in fully three-dimensional (3D) simulation, which because of numerical complexities are restricted to using a Newtonian constitutive equation. Further 2D modeling at nonisothermal conditions shows that the choice of representative Newtonian viscosity is dependent on the amount of heating of the initially room temperature mold. An early 3D transient model shows that the initial design of the distributor is sub-optimal. However, these simulations take several months to run on 4 processors of an HP workstation using a preconditioner/solver combination of ILUT/GMRES with fill factors of 3 and PSPG stabilization. Therefore, several modifications to the distributor geometry and orientations of the vents and molds have been investigated using much faster 3D steady-state simulations. The pressure distribution for these steady-state calculations is examined for three different distributor designs to see if this can indicate which geometry has the superior design. The second modification, with a longer distributor, is shown to have flatter, more monotonic isobars perpendicular to the flow direction indicating a better filling process. The effects of the distributor modifications, as well as effects of the mold orientation, have also been examined with laboratory experiments in which the flow of a viscous Newtonian oil entering transparent molds is recorded visually. Here, the flow front is flatter and voids are reduced for the second geometry compared to the original geometry. A horizontal orientation, as opposed to the planned vertical orientation, results in fewer voids. Recently, the Navier-Stokes equations have been stabilized with the Dohrman-Bochev PSPP stabilization method, allowing us to calculate transient 3D simulations with computational times on the order of days instead of months. Validation simulations are performed and compared to the experiments. Many of the trends of the experiments are captured by the level set modeling, though quantitative agreement is lacking mainly due to the high value of the gas phase viscosity necessary for numerical stability, though physically unrealistic. More correct trends are predicted for the vertical model than the horizontal model, which is serendipitous as the actual mold is held in a vertical geometry. The full, transient mold filling calculations indicate that the flow front is flatter and voids may be reduced for the second geometry compared to the original geometry. The validated model is used to predict mold filling for the actual process with the material properties for the PZT paste, the original distributor geometry, and the mold in a vertical orientation. This calculation shows that voids may be trapped at the four corners of the mold opposite the distributor.

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Thermal properties of PZT95/5(1.8Nb) and PSZT ceramics

Yang, Pin Y.; DiAntonio, Christopher D.; Burns, George B.; Rae, David F.

Thermal properties of niobium-modified PZT95/5(1.8Nb) and PSZT ceramics used for the ferroelectric power supply have been studied from -100 C to 375 C. Within this temperature range, these materials exhibit ferroelectric-ferroelectric and ferroelectric-paraelectric phase transformations. The thermal expansion coefficient, heat capacity, and thermal diffusivity of different phases were measured. Thermal conductivity and Grueneisen constant were calculated at several selected temperatures between -60 C and 100 C. Results show that thermal properties of these two solid solutions are very similar. Phase transformations in these ceramics possess first order transformation characteristics including thermal hysteresis, transformational strain, and enthalpy change. The thermal strain in the high temperature rhombohedral phase region is extremely anisotropic. The heat capacity for both materials approaches to 3R (or 5.938 cal/(g-mole*K)) near room temperature. The thermal diffusivity and the thermal conductivity are quite low in comparison to common oxide ceramics, and are comparable to amorphous silicate glass. Furthermore, the thermal conductivity of these materials between -60 C and 100 C becomes independent of temperature and is sensitive to the structural phase transformation. These phenomena suggest that the phonon mean free path governing the thermal conductivity in this temperature range is limited by the lattice dimensions, which is in good agreement with calculated values. Effects of small compositional changes and density/porosity variations in these ceramics on their thermal properties are also discussed. The implications of these transformation characteristics and unusual thermal properties are important in guiding processing and handling procedures for these materials.

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The effects of process parameters on injection-molded PZT ceramics part fabrication- compounding process rheology

Yang, Pin Y.; Mondy, L.A.; Burns, George B.

Solid solutions of lead-based perovskites are the backbone materials of the piezoelectric components for transducer, actuator, and resonator applications. These components, typically small in size, are fabricated from large sintered ceramic slugs using grinding and lapping processes. These operations increase manufacturing costs and produce a large hazardous waste stream, especially when component size decreases. To reduce costs and hazardous wastes associated with the production of these components, an injection molding technique is being investigated to replace the machining processes. The first step in the new technique is to compound an organic carrier with a ceramic powder. The organic carrier is a thermoplastic based system composed of a main carrier, a binder, and a surfactant. Understanding the rheology of the compounded material is necessary to minimize the creation of defects such as voids or cavities during the injection-molding process. An experiment was performed to model the effects of changes in the composition and processing of the material on the rheological behavior. Factors studied included: the surfactant of the organic carrier system, the solid loading of the compounded material, and compounding time. The effects of these factors on the viscosity of the material were investigated.

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Effects of niobium addition on microstructural and electrical properties of lead zirconate titanate solid solution (PZT 95/5)

Ceramic Engineering and Science Proceedings

Yang, Pin; Voigt, James A.; Rodriguez, Marko A.; Moore, Roger H.; Burns, George B.

The impacts of small niobium additions to processing, microstructure, and electrical properties in the Zr-rich lead zirconate titanate ceramics (PZT 95/5) were investigated. The influence of niobium content on dielectric responses and the characteristics of ferroelectric behaviors, as well as the relative phase stability and the hydrostatic pressure induced ferroelectric-to- antiferroelectric phase transformation are reported. Results indicate that increasing the niobium concentration in the solid solutions enhances densification, refines the microstructure, decreases dielectric constant and spontaneous polarization, and stabilizes the ferroelectric phase. The stabilization of ferroelectric phase with respect to the antiferroelectric phase near PZT 95/5 composition dramatically increases the pressure required for the ferroelectric-to-antiferroelectric phase transformation. These observations were correlated to the creation of A-site vacancies and a slight modification of the crystal structure. The importance of these composition-property relationships on device application will be presented.

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Microfabrication with femtosecond laser processing : (A) laser ablation of ferrous alloys, (B) direct-write embedded optical waveguides and integrated optics in bulk glasses

Burns, George B.; Palmer, Jeremy A.; Harris, Marc F.; McDaniel, Karen L.; Guo, Junpeng; Vawter, Gregory A.; Tallant, David T.; Griffith, M.L.; Luk, Ting S.

At Sandia National Laboratories, miniaturization dominates future hardware designs, and technologies that address the manufacture of micro-scale to nano-scale features are in demand. Currently, Sandia is developing technologies such as photolithography/etching (e.g. silicon MEMS), LIGA, micro-electro-discharge machining (micro-EDM), and focused ion beam (FIB) machining to fulfill some of the component design requirements. Some processes are more encompassing than others, but each process has its niche, where all performance characteristics cannot be met by one technology. For example, micro-EDM creates highly accurate micro-scale features but the choice of materials is limited to conductive materials. With silicon-based MEMS technology, highly accurate nano-scale integrated devices are fabricated but the mechanical performance may not meet the requirements. Femtosecond laser processing has the potential to fulfill a broad range of design demands, both in terms of feature resolution and material choices, thereby improving fabrication of micro-components. One of the unique features of femtosecond lasers is the ability to ablate nearly all materials with little heat transfer, and therefore melting or damage, to the surrounding material, resulting in highly accurate micro-scale features. Another unique aspect to femtosecond radiation is the ability to create localized structural changes thought nonlinear absorption processes. By scanning the focal point within transparent material, we can create three-dimensional waveguides for biological sensors and optical components. In this report, we utilized the special characteristics of femtosecond laser processing for microfabrication. Special emphasis was placed on the laser-material interactions to gain a science-based understanding of the process and to determine the process parameter space for laser processing of metals and glasses. Two areas were investigated, including laser ablation of ferrous alloys and direct-write optical waveguides and integrated optics in bulk glass. The effects of laser and environmental parameters on such aspects as removal rate, feature size, feature definition, and ablation angle during the ablation process of metals were studied. In addition, the manufacturing requirements for component fabrication including precision and reproducibility were investigated. The effect of laser processing conditions on the optical properties of direct-written waveguides and an unusual laser-induced birefringence in an optically isotropic glass are reported. Several integrated optical devices, including a Y coupler, directional coupler, and Mach-Zehnder interferometer, were made to demonstrate the simplicity and flexibility of this technique in comparison to the conventional waveguide fabrication processes.

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Study of methods for automated crack inspection of electrically poled piezoelectric ceramics

Burns, George B.; Yang, Pin Y.; Jokiel, Bernhard J.; Hwang, Stephen C.

The goal of this project was to identify a viable, non-destructive methodology for the detection of cracks in electrically poled piezoelectric ceramics used in neutron generator power supply units. The following methods were investigated: Impedance Spectroscopy, Scanning Acoustic Microscopy, Lock-in Thermography, Photo-acoustic Microscopy, and Scanned Vicinal Light. In addition to the exploration of these techniques for crack detection, special consideration was given to the feasibility of integrating these approaches to the Automatic Visual Inspection System (AVIS) that was developed for mapping defects such as chips, pits and voids in piezoelectric ceramic components. Scanned Vicinal Light was shown to be the most effective method of automatically detecting and quantifying cracks in ceramic components. This method is also very effective for crack detection in other translucent ceramics.

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Femtosecond laser-pulse-induced birefringence in optically isotropic glass

Journal of Applied Physics

Yang, Pin Y.; Burns, George B.; Guo, Junpeng; Luk, Ting S.; Vawter, Gregory A.

The optical birefringence in an isotropic glass medium was created by using a regeneratively amplified Ti:sapphire femtosecond laser. The regions between two crossed polarizers modified by the femtosecond laser shows bright transmission with respect to the dark background of the isotropic glass. It was found that the angular dependence of transmission through the laser-modified region was consistent with that of an optically birefringent material. It was also observed that the optical axes of laser-induced birefringence can be controlled by the polarization direction of the femtosecond laser.

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The effect of lead stoichiometry on the dielectric performance of niobium modified PZT 95/5 ceramics

Ceramic Transactions

Yang, Pin Y.; Voigt, James A.; Lockwood, Steven J.; Rodriguez, Marko A.; Burns, George B.; Watson, Chad S.

The electrical properties of lead zirconate titanate ceramics near the 95/5 composition are extremely sensitive to the chemical composition and processing conditions. To precisely control the lead stoichiometry in a solid solution has been a challenge because of lead volatility during high temperature sintering. In this study, we investigated the effect of the amount of lead in the solid solution on crystal structure, dielectric behavior, and phase transformation characteristics for chemically prepared niobium modified PZT 95/5 ceramics. Implications are important for process control and assurance of material performance.

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Field-induced strain associated with polarization reversal in a rhombohedral ferroelectric ceramic

Proposed for publication in the Journal of Material Research.

Yang, Pin Y.; Yang, Pin Y.; Burns, George B.; Rodriguez, Marko A.

The polarization reversal process in a rhombohedral ferroelectric ceramic material was investigated using field-induced strain measurements and texture development. Special attention was focused on the difference in the field-induced strains between the first quarter cycle and subsequent loading conditions. Results show that the initial field-induced strain is about twelve times greater than the subsequent strain, which immediately suggests that mechanisms involved in these conditions during the polarization reversal process are different. The difference in the magnitude of field-induced strain is discussed in terms of 180 degree and non-180 degree domain reorientation processes.

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37 Results
37 Results